三元共沸体系加盐萃取精馏的工艺研究
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摘要
本文针对乙酸甲酯—乙醇—水三元共沸体系，提出了加盐萃取精馏的工艺过程，并对盐的选择和萃取剂的选择方法进行了研究。
将Sander等提出的UNIQUAC模型扩展到三元共沸体系，采用Matlab软件编程，模拟了由离子Cl~-、Br~-、NO_3~-、CH_3COO~-、Li~+、Na~+、K~+和Ca~(2+)组成的16种盐对体系的影响。又以盐在溶剂中的溶解度为评定目标，选择合适的盐为醋酸钾。
利用计算机分子设计，以基团贡献模型为基础，建立了一套溶剂选择优化的方法。再根据相对挥发度、相对分子摩尔质量、熔点、沸点、共沸和稳定判断等几个方面为指标进行分子设计，选择出了合适的萃取剂为乙二醇。
本文还设计安装了一套实验室连续进料萃取装置进行工艺的验证实验，对萃取精馏和加盐萃取精馏工艺流程分别进行了验证，并对萃取剂的回收利用进行了实验，取得了良好的效果。实验结果表明，本工艺流程是切实可行的，可以将三元混和物完全分离提纯。
A new process of extraction distillation with salt was developed for the triple azeotropic system of methyl acetate-ethanol-water and the selective method of the solvent and salt were studied.
The effect of the ions such as Cl CH3COO Na+ K+ and Ca2+ upon the phase equilibrium was simulated by Matlab, in which the UNIQUAC model put forward by Sander was extended to that is brought out by Sander is extended to the triple azeotropic system. KAC was the fit salt.
A method of solvent selected and optimized on the base of Group Contribution Model was established, then according the relative volatility, relative molecular mole mass, melting point, boiling point, and so on to design the solvent molecular. Glycol was the fit solvent.
One set of extractive experiment equipment with continuously feed was designed and established to validate the extractive distillation and extractive distillation with salt. Good results of the two technology processes and the extractive solvent recycling experiment were gained respectively. The results proved the process was feasible and the triple azeotropic system could be completely distillated.
将Sander等提出的UNIQUAC模型扩展到三元共沸体系，采用Matlab软件编程，模拟了由离子Cl~-、Br~-、NO_3~-、CH_3COO~-、Li~+、Na~+、K~+和Ca~(2+)组成的16种盐对体系的影响。又以盐在溶剂中的溶解度为评定目标，选择合适的盐为醋酸钾。
利用计算机分子设计，以基团贡献模型为基础，建立了一套溶剂选择优化的方法。再根据相对挥发度、相对分子摩尔质量、熔点、沸点、共沸和稳定判断等几个方面为指标进行分子设计，选择出了合适的萃取剂为乙二醇。
本文还设计安装了一套实验室连续进料萃取装置进行工艺的验证实验，对萃取精馏和加盐萃取精馏工艺流程分别进行了验证，并对萃取剂的回收利用进行了实验，取得了良好的效果。实验结果表明，本工艺流程是切实可行的，可以将三元混和物完全分离提纯。
A new process of extraction distillation with salt was developed for the triple azeotropic system of methyl acetate-ethanol-water and the selective method of the solvent and salt were studied.
The effect of the ions such as Cl CH3COO Na+ K+ and Ca2+ upon the phase equilibrium was simulated by Matlab, in which the UNIQUAC model put forward by Sander was extended to that is brought out by Sander is extended to the triple azeotropic system. KAC was the fit salt.
A method of solvent selected and optimized on the base of Group Contribution Model was established, then according the relative volatility, relative molecular mole mass, melting point, boiling point, and so on to design the solvent molecular. Glycol was the fit solvent.
One set of extractive experiment equipment with continuously feed was designed and established to validate the extractive distillation and extractive distillation with salt. Good results of the two technology processes and the extractive solvent recycling experiment were gained respectively. The results proved the process was feasible and the triple azeotropic system could be completely distillated.
引文
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3．许其佑．有机化工分离工程．上海：华东化工学院出版社，1990．125
4．史季芬．多级分离过程——蒸馏、吸收、萃取、吸附．北京：化学工业出版社，1991．126
5．雷良桓，段占庭，徐永福．加盐萃取精馏的研究——叔丁醇纯化过程的开发。石油化工，1982，11：404
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13. Abrams D, Prausnitz J. Statistical thermodynamics of liquid mixtures: A new expression for the excess gibbs energy of partly or completely miscible systems. AIChE J., 1975,21:116
14．徐明忠．无限稀释活度系数的实验测定方法．许昌师专学报，1997，16(1)：31
15．顾正桂，赵维彭，郑英峨，等．用色谱筛选苯和噻吩萃取精馏分离的溶剂．化学工业与工程，1990，7(3)：52
16．郑英峨，赵连玉，赵维彭，等．C_9—DMP多元体系萃取蒸馏汽液平衡模型的研究．石油学报(石油化工)，1991，7(4)：77
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36. T.C.TAN. Model For Predicting The Effect of Dissolved Salt On The Vapour Liquid Equilibrium Of Solvent Mixture. Chem Eng Res Des, 1987,65(7):355-366
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42．王守玉，赵承卜．苯—正丙醇—氯化锂体系汽液平衡．化学工程，1991，19(2)：72-76
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44．王守玉．几种盐对氯仿—甲醇体系汽液平衡的效应．石油化工，1992，21(11)：737-740
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47．陆小华，张吕正等．电解质混和溶剂体系汽液平衡的推算．高校化学工程学报．1992，6(2)：97-104
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2．Perry．R．化学工程手册(下册)．北京：化学工业出版社，1993．13-84
3．许其佑．有机化工分离工程．上海：华东化工学院出版社，1990．125
4．史季芬．多级分离过程——蒸馏、吸收、萃取、吸附．北京：化学工业出版社，1991．126
5．雷良桓，段占庭，徐永福．加盐萃取精馏的研究——叔丁醇纯化过程的开发。石油化工，1982，11：404
6. Eckert, C. A., et al., AICHE.J. Measurement and Application of Limiting Activity Coefficients, 1981, (27),33-36.
7．金克新，赵传钧，马沛生．化工热力学．天津：天津大学出版社，1990．137
8. Elpinstill J, Winkle M. Prediction of infinite dilution activity coefficients for polar-polar binary systems. Ind. End. Chem. Process Des. Dev., 1968,7(2): 213
9. Thomas E, Eckert C.. Prediction of limiting activity coefficients by a modified separation of cohesive energy density model and UNIFAC. Ind. Eng. Chem. Process Des. Dev., 1984,23:194-209
10. Reid R, Prausnitz J, Ploing B. The properties of gases and liquids. Thirded, MCGRW-HILL,New York, 1987
11．斯坦利M．瓦拉斯，化工相平衡，北京：中国石化出版社，1991．193
12. Fredenslund A, Johns R,Prausnitz J. Group-contribution estimation of activity coefficients in nonideal liquid mixture. AIChE J., 1975,21:1086
13. Abrams D, Prausnitz J. Statistical thermodynamics of liquid mixtures: A new expression for the excess gibbs energy of partly or completely miscible systems. AIChE J., 1975,21:116
14．徐明忠．无限稀释活度系数的实验测定方法．许昌师专学报，1997，16(1)：31
15．顾正桂，赵维彭，郑英峨，等．用色谱筛选苯和噻吩萃取精馏分离的溶剂．化学工业与工程，1990，7(3)：52
16．郑英峨，赵连玉，赵维彭，等．C_9—DMP多元体系萃取蒸馏汽液平衡模型的研究．石油学报(石油化工)，1991，7(4)：77
17. Berg L. Separation of ethylbenzene from p- and m- xylene by extractive distillation using mixture of oxygenated organic compounds. AIChE J. 1983, 29:694
18. Berg L, Yeh A. Separation of m-xylene from o-xylene by extractive distillation. Chem. Eng. Comm. 1987,54:149
19. Fu-Ming Lee, Pahl R. Solvent screening study and conceptual extractive distillation process to produce anhydrous ethanol from fermentation broth. Ind. End. Chem. Process Des. Dev, 1985, 24:168-172
20. Fu-Ming Lee. Use of organic sulfones as the extractive distillation solvent for aromatics recovery. Ind. End. Chem. Process Des. Dev, 1986, 25:949-957
21．杨振生．萃取精馏溶剂的计算机辅助分子设计研究：[硕士学位论文]．保存地点：天津大学，1995
22．胡爱平，段占庭．气提法用于分离剂的研究．天然气化工，1993，18(1)：52
23. Venkatasubramanian V. Computer-Aided Molecular Design Using Genetic Algorithms. Comput. Chem. Eng., 1994,18(9): 833
24. Gani R, Brignole E. Molecular design of solvents for liquid extraction based on UNIFAC. Fluid Phase Equil, 1983, 13:331-340
25. Derringer G, Markham R. A computer-based methodology for matching polymer structures with required properties. Journal of Applied Polymer Science, 1985, 30:4609-4617
26. Gani R, Nielsen B, Fridenslund A. A Group Contribution Approach to computer-Aided Molecular Design. AIChE J, 1991, 37(9): 1318
27．倪力军，张立国，倪进方，等．链烷烃分子结构设计(Ⅰ)分子构成基团的确定．计算机与应用化学，1998，15(5)：298
28. Mathias P, Cheng H, Cook S, etal. Molecular Modeling in Engineering Design and Material development. Fluid Phase Equilibria, 1996,116:225
29. Evans L. Process modeling: what Lies Ahead. Chem. Eng. Progress, 1990,86:42
30．黄子卿．电解质溶液理论导论．科学出版社，1964
31. Frank J.Millero.The molal volumes of Electrolytes. Chemical Reviews, 1971, (2): 147-176
32. W.L.Wu, Y.M.Zhang,et. Modification of the Furter equation and correlation of the vapor-liquid equilibrium for mixed-solvent electrolyte systems. Fluid Phase Equilibria, 1999(154): 301-310
33. I-Min Shiah, Wen-Lu Weng, An activity coefficient model for predicting salt effects on vapor-liquid equilibria of mixed solvent systems. Fluid Phase Equilibria, 2000(70): 297-308
34. Chau-Chyun Chen, H.I.Britt, etal. Lacal Composition Model for Excess Gibbs Energy of Electrolyte Systems. AIChE J, 1982,28(4): 588-596
35. Rohini Badrayani, Anil Kumar. A Simple Model for Estimation of Activity Coefficient of Salts in Aqueous and Nonaqueous Solutions and Their Mixtures up to High Temperatures. Ind.Eng. Chem. Res.2001, 40:1996-2003
36. T.C.TAN. Model For Predicting The Effect of Dissolved Salt On The Vapour Liquid Equilibrium Of Solvent Mixture. Chem Eng Res Des, 1987,65(7):355-366
37．赵承卜，王守玉，韩丽君．汽液平衡盐效应的预测．化学工程，1986，1：71-78
38．孙仁义，张顺利．醇—水—盐体系汽液平衡数据关联．化学工程，1993，21(3)：59-63
39．陈新志，侯虞钧．含电解质体系的相平衡研究—用溶剂化方法关联含盐体系的汽液平衡．塑料新闻，1989，40(2)：203-212
40. D Jaques, Furter W F. Salt Effects in Vapor-Liquid Equilibrium:Testing the Thermodynamic consistency of Ethanol-Water Saturated with Inorganic Salts. AIChE J, 1972,18:343-346
41．赵承卜，李佛华，王守玉．环己烷—异丙醇含盐体系的汽液平衡．石油化工，1991，20(9)：617～621
42．王守玉，赵承卜．苯—正丙醇—氯化锂体系汽液平衡．化学工程，1991，19(2)：72-76
43．王守玉，蔡成良．乙酸甲酯—甲醇含盐体系汽液平衡．石油化工，1993，22(7)：444-450
44．王守玉．几种盐对氯仿—甲醇体系汽液平衡的效应．石油化工，1992，21(11)：737-740
45. Rousseau R W, Boone J E. Vapor-Liquid Equilibrium for Salt Containing Systems:Correlation of Binary Solvent Data and Prediction of Behavior in Multicomponent Solvents. AIChE J, 1978,24: 718-725
46．陈霭璠，罗瑞贤．含电解质的丙酮—水溶液的汽液平衡的近似计算．高校化学工程学报．1989，3(4)：28-33
47．陆小华，张吕正等．电解质混和溶剂体系汽液平衡的推算．高校化学工程学报．1992，6(2)：97-104
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